TW201736770A - Method of controlling pressure within a pressure vessel - Google Patents

Method of controlling pressure within a pressure vessel Download PDF

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TW201736770A
TW201736770A TW105142792A TW105142792A TW201736770A TW 201736770 A TW201736770 A TW 201736770A TW 105142792 A TW105142792 A TW 105142792A TW 105142792 A TW105142792 A TW 105142792A TW 201736770 A TW201736770 A TW 201736770A
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pressure
pressure vessel
vapor
kpa
reactor
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哈瑞許 派特爾
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薩比克全球科技公司
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/24Stationary reactors without moving elements inside
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B08CLEANING
    • B08BCLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B9/00Cleaning hollow articles by methods or apparatus specially adapted thereto 
    • B08B9/08Cleaning containers, e.g. tanks
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00162Controlling or regulating processes controlling the pressure
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00245Avoiding undesirable reactions or side-effects
    • B01J2219/00247Fouling of the reactor or the process equipment
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00245Avoiding undesirable reactions or side-effects
    • B01J2219/00254Formation of unwanted polymer, such as "pop-corn"

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Chemical Vapour Deposition (AREA)

Abstract

A method of controlling pressure within a pressure vessel includes introducing a flushing fluid stream into a pressure vessel, wherein the pressure vessel comprises a vapor injection valve and a vapor release valve; passing a first vapor stream through the vapor injection valve and into the pressure vessel when a pressure within the pressure vessel reaches a minimum value; passing a second vapor stream through the vapor release valve and out of the pressure vessel when the pressure within the pressure vessel reaches a maximum value, wherein the minimum value and the maximum value are different.

Description

控制壓力容器中的壓力之方法 Method of controlling pressure in a pressure vessel

本案係關於控制壓力容器中的壓力之方法。 This case relates to a method of controlling the pressure in a pressure vessel.

壓力容器被使用於各種工業及民營部門兩者的應用中。壓力容器出現在這些部門中作為工業壓縮空氣接受器及生活用熱水儲存槽。其他壓力容器的例子有潛水筒、再壓縮室、蒸餾塔、壓力反應器、高壓釜、及在採礦作業、煉油廠和石化工廠中的許多其他的容器、核反應器容器、潛艇和太空船居住艙、氣壓儲存器、壓力下的液壓油箱、軌道車空氣制動儲存器、道路車空氣制動儲存器、以及液化氣體(例如氨、氯、及液態石油氣)之儲存容器。 Pressure vessels are used in a variety of industrial and private sector applications. Pressure vessels appear in these sectors as industrial compressed air receivers and domestic hot water storage tanks. Examples of other pressure vessels are submersibles, recompression chambers, distillation columns, pressure reactors, autoclaves, and many other vessels in mining operations, refineries and petrochemical plants, nuclear reactor vessels, submarines and spacecraft cabins. , air pressure storage, hydraulic tank under pressure, rail car air brake storage, road vehicle air brake storage, and storage containers for liquefied gases (such as ammonia, chlorine, and liquid petroleum gas).

習知的壓力控制方法常常涉及非可變或靜壓力控制系統。每當達到一定內壓力值時,這些方法從容器中增加或釋放壓力。此壓力值為單一靜態值。這些靜態系統導致顯著缺乏效率及經濟損失。例如,必須非常頻繁地調整容器中的壓力。此導致壓力調整流的過度使用,並且也讓顯著量的儲存材料從容器逸出。 Conventional pressure control methods often involve non-variable or static pressure control systems. These methods increase or release pressure from the container whenever a certain internal pressure value is reached. This pressure value is a single static value. These static systems result in significant lack of efficiency and economic loss. For example, the pressure in the container must be adjusted very frequently. This results in overuse of the pressure regulating flow and also allows a significant amount of stored material to escape from the container.

特別是在與寡聚物及/或聚合物製造(例如乙烯之聚合、或乙烯之寡聚合,例如用於製造共聚單體級線性α-烯烴之選擇性乙烯二、三及四聚合)有關的技術中,設備積垢是個問題且經常遇到。在此類製程中,蠟和聚合物是不能被完全避免的固有副產物。這些蠟和聚合物可導致反應器本身以及周邊和下游設備的積垢。在最差的情況下,部分的設備,例如管,在隨後的製程區段中被堵塞,後果是必須將該製程關閉。 In particular in connection with the manufacture of oligomers and/or polymers (for example, polymerization of ethylene, or oligomerization of ethylene, for example, selective ethylene di-, tri- and tetra-polymerization for the production of comonomer-grade linear alpha-olefins) In technology, equipment fouling is a problem and is often encountered. In such processes, waxes and polymers are inherent by-products that cannot be completely avoided. These waxes and polymers can cause fouling of the reactor itself as well as surrounding and downstream equipment. In the worst case, some of the equipment, such as the pipe, is blocked in the subsequent process section, with the consequence that the process must be shut down.

在乙烯及/或其他α-烯烴之聚合中,聚合物固體的沉積亦可發生在具有各種壓力變化的反應器及/或設備中。 In the polymerization of ethylene and/or other alpha-olefins, the deposition of polymer solids can also occur in reactors and/or equipment having various pressure variations.

為了控制聚合物和蠟的沉積物,反應器必須定期清潔。為了避免任何長的停工期間,需要備用反應器來防止任何的製造損失。 In order to control the deposit of polymer and wax, the reactor must be cleaned regularly. In order to avoid any long downtime, an alternate reactor is required to prevent any manufacturing losses.

關於清潔帶有固體沉積物(例如高分子量寡聚物/聚合物)的反應器,反應器到目前為止必須要被打開,且通常工廠人員必須進入反應器來機械清潔。在清潔後,必須使反應器再次成為惰性的。原因是任何微量的水分及氧將毒化用於寡聚合和聚合的高敏感性有機金屬觸媒。此程序非常耗時。總之,典型的反應器停工時間為約1星期或更長,導致相當大的總生產率損失。 With regard to cleaning reactors with solid deposits (e.g., high molecular weight oligomers/polymers), the reactor must be opened to date, and typically the plant personnel must enter the reactor for mechanical cleaning. After cleaning, the reactor must be rendered inert again. The reason is that any traces of moisture and oxygen will poison the highly sensitive organometallic catalyst used for oligomerization and polymerization. This program is very time consuming. In summary, typical reactor downtimes are about one week or longer, resulting in considerable total productivity loss.

為了克服這些缺點,用來避免任何機械清潔的程序包括將具有溫度為至少約75℃的熱溶劑導入反應器以溶解聚合物沉積物。於清潔後,該溶劑可,例如藉由蒸 餾、結晶、薄膜蒸發、刮膜蒸發(wiped-film evaporation)及/或降膜蒸發,於溶劑回收單元中回收。 To overcome these disadvantages, procedures for avoiding any mechanical cleaning include introducing a hot solvent having a temperature of at least about 75 ° C into the reactor to dissolve the polymer deposits. After cleaning, the solvent can be, for example, steamed Distillation, crystallization, thin film evaporation, wiped-film evaporation, and/or falling film evaporation are recovered in a solvent recovery unit.

只要聚合物固體材料具有足夠短的碳鏈長的特點,此方法就會以令人滿意的方式作用。這對使用鋯系觸媒系統(其通常僅提供相對短的鏈長之聚乙烯和蠟)尤為主此。然而,若微量級雜質經固有地(經由原料雜質)或非故意地(由失穩製程條件所導致)導入到寡聚合反應器,則會改變此情況。尤其是微量的水分、空氣及/或腐蝕生成物可誘導在芳族溶劑中溶解性相對差的長鏈及潛在的支鏈聚乙烯的形成。 This method works in a satisfactory manner as long as the polymer solid material has a sufficiently short carbon chain length. This is especially true for zirconium-based catalyst systems, which typically only provide relatively short chain lengths of polyethylene and wax. However, this can be changed if trace levels of impurities are introduced intrinsically (via raw material impurities) or unintentionally (caused by destabilizing process conditions) into the oligomerization reactor. In particular, traces of moisture, air and/or corrosion products can induce the formation of relatively long-chain and potentially branched polyethylenes that are relatively poorly soluble in aromatic solvents.

使用其他觸媒系統,例如鉻系觸媒系統於乙烯之選擇性三或四聚合,會大幅加劇此情況。雖然在符合規格的情況下只有微量的聚乙烯形成,Cr誘導的聚合物傾向具有較長的鏈長及大幅減緩溶解過程之形態學的特徵。 The use of other catalyst systems, such as chromium-based catalyst systems, for selective three or four polymerization of ethylene can greatly exacerbate this situation. Although only a small amount of polyethylene is formed in compliance with specifications, Cr-induced polymers tend to have longer chain lengths and greatly slow the morphological characteristics of the dissolution process.

習知在沖洗系統中之壓力控制方法涉及非可變或靜壓力控制系統。每當達到一定內壓力值時,這些方法從容器中增加或釋放壓力。此等靜態系統導致顯著缺乏效率及經濟損失。例如,必須非常頻繁地調整容器中的壓力。此導致壓力調整流的過度使用,並且也讓顯著量的儲存材料從容器逸出。 Conventional pressure control methods in irrigation systems involve non-variable or static pressure control systems. These methods increase or release pressure from the container whenever a certain internal pressure value is reached. These static systems result in significant lack of efficiency and economic loss. For example, the pressure in the container must be adjusted very frequently. This results in overuse of the pressure regulating flow and also allows a significant amount of stored material to escape from the container.

因此,需要有效的控制壓力容器中之壓力的方法,其顯著地減少壓力調整流的使用及因頻繁的壓力調整所損失的儲存材料量。 Accordingly, there is a need for a method of effectively controlling the pressure in a pressure vessel that significantly reduces the use of pressure regulating flow and the amount of stored material lost due to frequent pressure adjustments.

在各個具體態樣中揭示了控制壓力容器中的壓力之方法以及沖洗反應器之方法。 Methods of controlling the pressure in a pressure vessel and methods of flushing the reactor are disclosed in various specific aspects.

控制壓力容器中的壓力之方法,包含:將沖洗流體流導入壓力容器,其中該壓力容器包含蒸氣注入閥和蒸氣釋放閥;當該壓力容器中的壓力達到最小值時,將第一蒸氣流通過該蒸氣注入閥並進入到該壓力容器中;當該壓力容器中的壓力達到最大值時,將第二蒸氣流通過該蒸氣釋放閥並離開該壓力容器,其中該最小值和該最大值是不同的。 A method of controlling pressure in a pressure vessel, comprising: introducing a flow of a flushing fluid into a pressure vessel, wherein the pressure vessel comprises a vapor injection valve and a vapor release valve; and when the pressure in the pressure vessel reaches a minimum, passing the first vapor stream The vapor is injected into the valve and into the pressure vessel; when the pressure in the pressure vessel reaches a maximum, the second vapor stream is passed through the vapor release valve and exits the pressure vessel, wherein the minimum value and the maximum value are different of.

沖洗反應器之方法,包含:將沖洗流體流導入壓力容器,其中該壓力容器包含蒸氣注入閥和蒸氣釋放閥;當該壓力容器中的壓力達到最小值時,將第一蒸氣流通過該蒸氣注入閥並進入到該壓力容器中;當該壓力容器中的壓力達到最大值時,將第二蒸氣流通過該蒸氣釋放閥並離開該壓力容器,其中該最小值和該最大值是不同的;自該壓力容器抽出一部分該沖洗流體流;及將該部分沖洗流體流通過反應器以沖洗該反應器。 A method of rinsing a reactor, comprising: introducing a flow of a flushing fluid into a pressure vessel, wherein the pressure vessel comprises a vapor injection valve and a vapor release valve; and when the pressure in the pressure vessel reaches a minimum, the first vapor stream is injected through the vapor The valve enters the pressure vessel; when the pressure in the pressure vessel reaches a maximum, the second vapor stream is passed through the vapor release valve and exits the pressure vessel, wherein the minimum value and the maximum value are different; The pressure vessel draws a portion of the flushing fluid stream; and the portion of the flushing fluid stream is passed through the reactor to flush the reactor.

這些及其他的特點及特徵在下面被更詳細地描述。 These and other features and features are described in more detail below.

10‧‧‧壓力控制方法 10‧‧‧ Pressure control method

12‧‧‧流體沖洗流 12‧‧‧ fluid flushing flow

14‧‧‧壓力容器 14‧‧‧ Pressure vessel

16‧‧‧第一蒸氣流 16‧‧‧First vapor stream

18‧‧‧蒸氣注入閥 18‧‧‧Vapor injection valve

20‧‧‧第二蒸氣流 20‧‧‧Second vapor flow

22‧‧‧蒸氣釋放閥 22‧‧‧Vapor release valve

24‧‧‧合併線 24‧‧‧ merged line

26‧‧‧泵 26‧‧‧ pump

28‧‧‧加熱器 28‧‧‧heater

30‧‧‧流量控制器 30‧‧‧Flow controller

32‧‧‧反應器 32‧‧‧Reactor

以下是圖式之簡單說明,其中類似元件係經相似地編號,且其提出係出於闡明本文中所揭示之例示性具 體態樣的目的,而不是對其加以限制的目的。 The following is a brief description of the drawings in which like elements are numbered similarly and are presented for the purpose of illustrating the exemplary embodiments disclosed herein. The purpose of the body, not the purpose of limiting it.

圖1為表示根據本揭示之壓力控制方法的簡化示意圖。 1 is a simplified schematic diagram showing a pressure control method in accordance with the present disclosure.

本文中所揭示的方法可提供有效控制壓力容器中的壓力之方法,其減少壓力調整流的使用及因頻繁的壓力調整而損失的儲存材料量。例如,本文中所揭示的方法可包括可變壓力控制系統。例如,該方法可包括在二組最小和最大點之間使用可變壓力。此與靜壓力相比可以是有利的,因為使用靜壓力通常導致使用更多的氮,而且當打開及關閉壓力閥來平衡靜壓力時會損失更多的甲苯。以本發明之方法,可使用除了靜態控制外之不同的控制類型來減少因壓力調整而損失的儲存材料量。該方法可減少需要的壓力調整的頻率。所揭示的方法可減少為了壓力調整之目的注入到壓力容器的材料量。例如,本文中所揭示的方法可減少所消耗的氮量大於或等於90%。該方法亦可減少在頻繁的壓力調整期間自容器損失的儲存材料量。例如,本文中所揭示的方法可減少自壓力容器損失的甲苯量大於或等於45%。 The methods disclosed herein provide a means of effectively controlling the pressure in a pressure vessel that reduces the use of pressure regulating flow and the amount of stored material that is lost due to frequent pressure adjustments. For example, the methods disclosed herein can include a variable pressure control system. For example, the method can include using a variable pressure between the two sets of minimum and maximum points. This can be advantageous compared to static pressure because the use of static pressure typically results in the use of more nitrogen, and more toluene is lost when the pressure valve is opened and closed to balance the static pressure. With the method of the present invention, different control types than static control can be used to reduce the amount of stored material lost due to pressure adjustment. This method reduces the frequency of pressure adjustments required. The disclosed method reduces the amount of material injected into the pressure vessel for pressure adjustment purposes. For example, the methods disclosed herein can reduce the amount of nitrogen consumed by greater than or equal to 90%. This method also reduces the amount of stored material lost from the container during frequent pressure adjustments. For example, the methods disclosed herein can reduce the amount of toluene lost from the pressure vessel by greater than or equal to 45%.

本文中所揭示的壓力控制方法可包括將沖洗流體流導入壓力容器。該壓力容器可包含蒸氣注入閥和蒸氣釋放閥。然後可在該壓力容器中的壓力達到最小值時,將第一蒸氣流通過該蒸氣注入閥並進入到該壓力容器中。當 該壓力容器中的壓力達到最大值時,可將第二蒸氣流通過該蒸氣釋放閥釋放並離開該壓力容器。該最小值和該最大值可以是相同或是不同的。可將一部分該沖洗流體流自該壓力容器抽出,並通過反應器來沖洗該反應器。 The pressure control method disclosed herein can include introducing a flow of irrigation fluid into a pressure vessel. The pressure vessel can include a vapor injection valve and a vapor release valve. The first vapor stream can then be passed through the vapor injection valve and into the pressure vessel when the pressure in the pressure vessel reaches a minimum. when When the pressure in the pressure vessel reaches a maximum, a second vapor stream can be released through the vapor release valve and exit the pressure vessel. The minimum and the maximum may be the same or different. A portion of the flushing fluid stream can be withdrawn from the pressure vessel and flushed through the reactor.

本文中所揭示的壓力控制方法可包括流體流。例如該流體流可包含溶劑,例如芳族溶劑。例如,該流體流可包含甲苯,用作為寡聚合反應中的溶劑。該流體流可包含沖洗流體。例如,該流體流可包含甲苯,用於沖洗反應器和熱交換器。該沖洗流體流可包含任何芳族溶劑。該流體流可包含任何在大氣壓力下具有沸點低於或等於300℃之有機液體。例如,該流體流可包含芳族溶劑、沸點低於或等於300℃之有機液體、或包含至少一種前述物之組合。 The pressure control methods disclosed herein can include fluid flow. For example, the fluid stream can comprise a solvent, such as an aromatic solvent. For example, the fluid stream can comprise toluene as a solvent in the oligomerization reaction. The fluid stream can comprise a flushing fluid. For example, the fluid stream can comprise toluene for flushing the reactor and heat exchanger. The flushing fluid stream can comprise any aromatic solvent. The fluid stream can comprise any organic liquid having a boiling point of less than or equal to 300 ° C at atmospheric pressure. For example, the fluid stream can comprise an aromatic solvent, an organic liquid having a boiling point of less than or equal to 300 ° C, or a combination comprising at least one of the foregoing.

本文中所描述的壓力控制方法可包括壓力容器。例如,可將流體流通過該壓力容器。例如,該壓力容器可為甲苯儲存容器。該壓力容器可包含鋼、複合材料、聚合物材料、或包含至少一種前述物之組合。容器中的溫度可大於或等於50℃。例如容器中的溫度可大於或等於80℃。例如,容器中的溫度可為80℃至250℃。該壓力容器可包含閥。例如,該壓力容器可包含多於或等於一個閥。例如,該壓力容器可包含2個閥。該閥可為注入閥、釋放閥或包含至少一種前述物之組合。例如,該壓力容器可包含一個注入閥和一個擴口洩壓閥(flare depressurization valve)。 The pressure control method described herein can include a pressure vessel. For example, a fluid stream can be passed through the pressure vessel. For example, the pressure vessel can be a toluene storage vessel. The pressure vessel can comprise steel, a composite material, a polymeric material, or a combination comprising at least one of the foregoing. The temperature in the container can be greater than or equal to 50 °C. For example, the temperature in the container can be greater than or equal to 80 °C. For example, the temperature in the container can range from 80 °C to 250 °C. The pressure vessel can contain a valve. For example, the pressure vessel can contain more than or equal to one valve. For example, the pressure vessel can contain 2 valves. The valve can be an injection valve, a release valve, or a combination comprising at least one of the foregoing. For example, the pressure vessel can include an injection valve and a flare depressurization valve.

本文中所揭示的壓力控制方法可包括將料流通過閥並進入到壓力容器中。例如,可將蒸氣流通過蒸氣注入閥並進入到壓力容器中。該蒸氣流可包含惰性氣體。例如,該蒸氣流可包含氮氣、甲烷氣、乙烷氣、或包含至少一種前述物之組合。當壓力容器中的壓力達到最小值時,可將該蒸氣流通過注入閥並進入到壓力容器中。該蒸氣流之注入可增加壓力容器中的壓力。 The pressure control method disclosed herein can include passing a stream through a valve and into a pressure vessel. For example, a vapor stream can be passed through a vapor injection valve and into a pressure vessel. The vapor stream can comprise an inert gas. For example, the vapor stream can comprise nitrogen, methane gas, ethane gas, or a combination comprising at least one of the foregoing. When the pressure in the pressure vessel reaches a minimum, the vapor stream can be passed through an injection valve and into the pressure vessel. The injection of this vapor stream increases the pressure in the pressure vessel.

本文中所揭示的壓力控制方法可包括將料流通過閥,將該料流自壓力容器釋放。例如,可將蒸氣流通過擴口洩壓閥,將該蒸氣流自壓力容器釋放。自壓力容器釋放的蒸氣流可包含氣相的被儲存在壓力容器中之流體、惰性氣體、或包含至少一種前述物之組合。例如,自壓力容器釋放的蒸氣流可包含氮氣及氣相甲苯。當壓力容器中的壓力達到最大值時,可將蒸氣流通過擴口洩壓閥自壓力容器釋放。該蒸氣流的釋放可降低壓力容器中的壓力。 The pressure control method disclosed herein can include passing a stream through a valve to release the stream from a pressure vessel. For example, the vapor stream can be passed through a flared pressure relief valve to release the vapor stream from the pressure vessel. The vapor stream released from the pressure vessel may comprise a fluid in the gas phase that is stored in the pressure vessel, an inert gas, or a combination comprising at least one of the foregoing. For example, the vapor stream released from the pressure vessel can comprise nitrogen and gaseous toluene. When the pressure in the pressure vessel reaches a maximum, the vapor stream can be released from the pressure vessel through a flared pressure relief valve. The release of this vapor stream reduces the pressure in the pressure vessel.

本文中所揭示的壓力控制方法可包括可變、非靜壓力控制系統。例如,壓力容器中的最小壓力值和最大壓力值可以是不同的數值。例如,最小壓力值可為10千帕至500千帕。例如,最小壓力值可為300千帕至400千帕。例如,最小壓力值可為350千帕。最大壓力值可為50千帕至1000千帕。例如,最大壓力值可為600千帕至700千帕。例如,最大壓力值可為650千帕。最小壓力值和最大壓力值可相差,例如,大於或等於10千帕。例如,該等數值可相差大於或等於300千帕。 The pressure control methods disclosed herein can include variable, non-static pressure control systems. For example, the minimum pressure value and the maximum pressure value in the pressure vessel can be different values. For example, the minimum pressure value can range from 10 kPa to 500 kPa. For example, the minimum pressure value can range from 300 kPa to 400 kPa. For example, the minimum pressure value can be 350 kPa. The maximum pressure can range from 50 kPa to 1000 kPa. For example, the maximum pressure value can range from 600 kPa to 700 kPa. For example, the maximum pressure value can be 650 kPa. The minimum pressure value and the maximum pressure value may differ by, for example, greater than or equal to 10 kPa. For example, the values can differ by more than or equal to 300 kPa.

本文中所揭示的壓力控制方法可包括將流體流自壓力容器抽出。例如,本文中所揭示的方法可包含將包含甲苯之沖洗流體流自壓力容器抽出。該流體流可通過多於或等於一個泵。例如,該流體流可藉由多於或等於一個泵推進。例如,該流體流可藉由2個泵推進。該泵可獨立於壓力容器中的壓力操作。例如,泵吸入壓力的變化將不會影響自壓力容器抽出之流體流的流量(壓力容器中壓力的變化亦對泵之性能沒有影響)。該流體流可通過熱交換器。例如,可將流體流通過加熱器便可增加該流體流的溫度。 The pressure control method disclosed herein can include withdrawing a fluid stream from a pressure vessel. For example, the methods disclosed herein can include withdrawing a stream of flushing fluid comprising toluene from a pressure vessel. The fluid stream can pass more than or equal to one pump. For example, the fluid stream can be propelled by more than or equal to one pump. For example, the fluid stream can be propelled by 2 pumps. The pump can be operated independently of the pressure in the pressure vessel. For example, changes in pump suction pressure will not affect the flow of fluid from the pressure vessel (changes in pressure in the pressure vessel also have no effect on pump performance). This fluid stream can pass through a heat exchanger. For example, the fluid stream can be passed through a heater to increase the temperature of the fluid stream.

本文中所揭示的壓力控制方法,可包括將流體流通過反應器或熱交換器用於沖洗的目的。該流體流可用作為溶劑流。例如,該流體流可用作為寡聚合反應器之溶劑流。該流體流可在通過反應器或熱交換器後回到壓力容器作為閉環系統的一部分。流體流的流量可由流量控制器控制。 The pressure control methods disclosed herein can include the purpose of passing a fluid stream through a reactor or heat exchanger for rinsing. This fluid stream can be used as a solvent stream. For example, the fluid stream can be used as a solvent stream for the oligomerization reactor. The fluid stream can be returned to the pressure vessel as part of a closed loop system after passing through the reactor or heat exchanger. The flow of fluid flow can be controlled by a flow controller.

本方法可用來清潔用於寡聚合或聚合的反應器及/或設備。寡聚合應包含烯烴,例如乙烯,之二、三及四聚合以製造直鏈α-烯烴。聚合包括乙烯及其他α-烯烴之聚合以及其共聚合。 The process can be used to clean reactors and/or equipment for oligomerization or polymerization. The oligomeric polymerization should comprise an olefin, such as ethylene, which is polymerized in two, three and four to produce a linear alpha olefin. Polymerization includes the polymerization of ethylene and other alpha-olefins as well as their copolymerization.

在寡聚合中,聚合物殘渣係固有地形成作為副產物,其可在反應器及/或設備中形成沉積物。在聚合過程中,產物本身(聚合物)可形成各自的沉積物。在寡聚合及聚合二者的過程中,反應器及/或設備皆必須被清潔以 避免其堵塞。 In oligomeric polymerization, polymer residues are inherently formed as by-products that can form deposits in the reactor and/or equipment. During the polymerization, the product itself (polymer) can form its own deposit. In both the oligomerization and polymerization processes, the reactor and/or equipment must be cleaned to Avoid blocking it.

藉由參照所附圖式,可獲得對本文中所揭示之組件、方法、及器械之更完整的理解。這些圖式(在本文中亦稱為“圖”)僅為基於說明本揭露之方便性及容易性的示意圖示,因此並無意欲指出裝置其組件之相對大小及尺寸及/或界定或限制例示性具體態樣的範圍。雖然為了明確性在下面的說明中使用了特定術語,但是這些術語意圖僅指圖式中被選擇用來說明的具體態樣之特定結構,而不欲界定或限制本揭露的範圍。在下面之圖式及以下說明中,應理解相似數字標號係指具有相似功能的組件。 A more complete understanding of the components, methods, and instrumentologies disclosed herein can be obtained by reference to the accompanying drawings. The drawings (also referred to herein as "figure") are merely schematic representations based on the convenience and ease of illustration of the present disclosure, and thus are not intended to indicate the relative size and size and/or definition or limitation of the components of the device. Illustrative range of specific aspects. The specific terminology used in the following description is for the purpose of illustration and description In the following figures and the following description, it should be understood that like reference numerals refer to the

現參考圖1,本文中所揭示的壓力控制方法10可包括將流體沖洗流12通過壓力容器14。例如,流體沖洗流12可包含甲苯而壓力容器14可為甲苯儲存容器。本文中所揭示的方法可包括將第一蒸氣流16通過蒸氣注入閥18。例如,第一蒸氣流16可包含氮。可將第一蒸氣流16通過蒸氣注入閥18並經由合併線24進入到壓力容器14中。例如,當壓力容器14中的壓力達到最小值時,可將第一蒸氣流16通入壓力容器14。 Referring now to FIG. 1, the pressure control method 10 disclosed herein can include passing a fluid flushing stream 12 through a pressure vessel 14. For example, fluid flushing stream 12 can comprise toluene and pressure vessel 14 can be a toluene storage vessel. The method disclosed herein can include passing the first vapor stream 16 through a vapor injection valve 18. For example, the first vapor stream 16 can comprise nitrogen. The first vapor stream 16 can be passed through the vapor injection valve 18 and into the pressure vessel 14 via the merge line 24. For example, the first vapor stream 16 can be passed to the pressure vessel 14 when the pressure in the pressure vessel 14 reaches a minimum.

本文中所揭示的壓力控制方法可包括將第二蒸氣流20通過蒸氣釋放閥22。例如,第二蒸氣流20可包含氣態氮及及氣態甲苯。例如,第二蒸氣流20可經由合併線24離開壓力容器14然後通過蒸氣釋放閥22。例如,當壓力容器14中的壓力達到最大值時,第二蒸氣流20可離開壓力容器14。例如,該最大壓力值和最小壓力 值可為不同的數值。 The pressure control method disclosed herein can include passing the second vapor stream 20 through the vapor release valve 22. For example, the second vapor stream 20 can comprise gaseous nitrogen and gaseous toluene. For example, the second vapor stream 20 can exit the pressure vessel 14 via the merge line 24 and then pass through the vapor release valve 22. For example, the second vapor stream 20 can exit the pressure vessel 14 when the pressure in the pressure vessel 14 reaches a maximum. For example, the maximum pressure value and the minimum pressure Values can be different values.

本文中所揭示的壓力控制方法可包括自壓力容器14抽出流體沖洗流12。然後可將流體沖洗流12通過泵26。例如,流體沖洗流12可藉由泵26推進。泵26可獨立於壓力容器14中的壓力操作。亦可將流體沖洗流12通過加熱器28。壓力控制方法10可為閉環系統。 The pressure control method disclosed herein can include withdrawing the fluid flushing stream 12 from the pressure vessel 14. Fluid flushing stream 12 can then be passed through pump 26. For example, fluid flushing stream 12 can be propelled by pump 26. Pump 26 can operate independently of the pressure in pressure vessel 14. Fluid flushing stream 12 can also be passed through heater 28. The pressure control method 10 can be a closed loop system.

本文中所揭示的壓力控制方法可包括將流體沖洗流12通過反應器32以沖洗反應器32。流體沖洗流12流到反應器32的流量可藉由流量控制器30控制。流體沖洗流12可通過反應器32然後回饋到壓力容器14成為閉環壓力控制方法10的一部分。 The pressure control method disclosed herein can include passing a fluid flushing stream 12 through reactor 32 to flush reactor 32. The flow of fluid flushing stream 12 to reactor 32 can be controlled by flow controller 30. The fluid flushing stream 12 can be passed through the reactor 32 and then fed back to the pressure vessel 14 as part of the closed loop pressure control method 10.

下列實施例僅係說明本文中所揭示之壓力控制方法,而不意欲限制其範圍。 The following examples are merely illustrative of the pressure control methods disclosed herein and are not intended to limit the scope thereof.

實施例 Example 比較實施例1 Comparative Example 1

習知的壓力容器中之壓力控制方法係用於本比較實施例的目的。使用了靜態、非可變壓力控制系統。在510千帕的固定壓力下操作甲苯儲存壓力容器。將氮注入到容器中以增加容器中的壓力,而將釋放閥打開以降低壓力。使用此方法進行二個獨立的試驗,試驗1及試驗2。試驗係相隔一個月進行。二個試驗的結果描述於表1。所消耗的總氮量以每天的公斤數表示。總通氣流量以每天的公斤數表示。甲苯濃度以質量百分比表示。所消耗的甲苯 總量以每天的公斤數表示。溫度保持持恆定在155℃。 Pressure control methods in conventional pressure vessels are used for the purposes of this comparative example. A static, non-variable pressure control system is used. The toluene storage pressure vessel was operated at a fixed pressure of 510 kPa. Nitrogen is injected into the container to increase the pressure in the container, while the release valve is opened to reduce the pressure. Two separate tests, Test 1 and Test 2, were performed using this method. The test was conducted one month apart. The results of the two tests are described in Table 1. The total amount of nitrogen consumed is expressed in kilograms per day. The total ventilation flow is expressed in kilograms per day. The toluene concentration is expressed in mass percent. Toluene consumed The total amount is expressed in kilograms per day. The temperature was held constant at 155 °C.

實施例1 Example 1

根據本揭露的壓力控制方法,及如圖1所描述,係用於本實施例的目的。使用了可變、非靜壓力控制系統。用氮的注入來增加甲苯容器中的壓力。使用壓力釋放閥來降低壓力。最大壓力值係設在650千帕,且最小壓力值係設在350千帕。容器可用的淨正吸高差為20公尺,而所需淨正吸高差為5.3公尺。容器中的溫度為155℃。結果描述於表1作為試驗3。可看出,本文中所揭示的方法(試驗3)顯著地減少為了壓力調整之目的須注入到壓力容器的材料量(與試驗1及試驗2相比)。例如,本文中所揭示的方法可減少所消耗的氮量大於或等於90%。本文中所揭示的方法亦可顯著地減少在頻繁的壓力調整期間自容器損失的儲存材料量。例如,本文中所揭示的方法可減少自壓力容器損失的甲苯量大於或等於45%。 The pressure control method according to the present disclosure, as described in FIG. 1, is used for the purpose of the present embodiment. A variable, non-static pressure control system is used. Nitrogen injection is used to increase the pressure in the toluene vessel. Use a pressure relief valve to reduce pressure. The maximum pressure is set at 650 kPa and the minimum pressure is set at 350 kPa. The net positive suction height difference of the container is 20 meters, and the required net positive suction height difference is 5.3 meters. The temperature in the vessel was 155 °C. The results are described in Table 1 as Test 3. It can be seen that the method disclosed herein (Test 3) significantly reduces the amount of material that must be injected into the pressure vessel for pressure adjustment purposes (compared to Test 1 and Test 2). For example, the methods disclosed herein can reduce the amount of nitrogen consumed by greater than or equal to 90%. The methods disclosed herein can also significantly reduce the amount of stored material lost from the container during frequent pressure adjustments. For example, the methods disclosed herein can reduce the amount of toluene lost from the pressure vessel by greater than or equal to 45%.

本文中所揭露的方法包括至少下列具體態樣: The methods disclosed herein include at least the following specific aspects:

具體態樣1:一種控制壓力容器中的壓力之方法,其包含:將沖洗流體流導入壓力容器,其中該壓力容器包含蒸氣注入閥和蒸氣釋放閥;當該壓力容器中的壓力達到最小值時,將第一蒸氣流通過該蒸氣注入閥並進入到該壓力容器中;及當該壓力容器中的壓力達到最大值時,將第二蒸氣流通過該蒸氣釋放閥並離開該壓力容器,其中該最小值和該最大值是不同的。 Aspect 1: A method of controlling pressure in a pressure vessel, comprising: introducing a flow of a flushing fluid into a pressure vessel, wherein the pressure vessel comprises a vapor injection valve and a vapor release valve; when the pressure in the pressure vessel reaches a minimum value Passing a first vapor stream through the vapor injection valve and into the pressure vessel; and when the pressure in the pressure vessel reaches a maximum, passing a second vapor stream through the vapor release valve and exiting the pressure vessel, wherein The minimum value and the maximum value are different.

具體態樣2:如具體態樣1之方法,其中該沖洗流體流包含芳族溶劑、沸點低於或等於300℃之有機液體、或包含至少一種前述物之組合,較佳者為其中該沖洗流體包含甲苯。 2: The method of the specific aspect 1, wherein the rinsing fluid stream comprises an aromatic solvent, an organic liquid having a boiling point lower than or equal to 300 ° C, or a combination comprising at least one of the foregoing, preferably wherein the rinsing The fluid contains toluene.

具體態樣3:如前述具體態樣中任一者之方法,其中該第一蒸氣流包含惰性氣體,較佳者為其中該第一蒸氣流包含氮氣、甲烷氣、乙烷氣、或包含至少一種前述物之組合。 The method of any one of the preceding aspects, wherein the first vapor stream comprises an inert gas, preferably wherein the first vapor stream comprises nitrogen, methane, ethane, or at least A combination of the foregoing.

具體態樣4:如前述申請專利範圍中任一者之方法,其中該第二蒸氣流包含呈氣相之該沖洗流體。 The method of any one of the preceding claims, wherein the second vapor stream comprises the flushing fluid in a gas phase.

具體態樣5:如前述具體態樣中任一者之方法,其中該壓力容器中的溫度為80℃至250℃。 The method of any one of the preceding aspects, wherein the temperature in the pressure vessel is from 80 ° C to 250 ° C.

具體態樣6:如前述具體態樣中任一者之方法,其中該壓力容器中的壓力的最小值為10千帕至500千帕。 The method of any one of the preceding aspects, wherein the pressure in the pressure vessel has a minimum value of from 10 kPa to 500 kPa.

具體態樣7:如前述具體態樣中任一者之方 法,其中該壓力容器中的壓力的最大值為50千帕至1000千帕。 Concrete aspect 7: Any of the foregoing specific aspects The method wherein the pressure in the pressure vessel has a maximum value of from 50 kPa to 1000 kPa.

具體態樣8:如前述具體態樣中任一者之方法,其中該壓力容器中的壓力的最小值與該壓力容器中的壓力的最大值相差大於或等於10千帕。 The method of any one of the preceding aspects, wherein the minimum value of the pressure in the pressure vessel differs from the maximum value of the pressure in the pressure vessel by greater than or equal to 10 kPa.

具體態樣9:如前述具體態樣中任一者之方法,其中該沖洗流體流係藉由泵推進,其中該泵獨立於該壓力容器中的壓力操作。 A method of any one of the preceding aspects, wherein the flushing fluid stream is propelled by a pump, wherein the pump operates independently of the pressure in the pressure vessel.

具體態樣10:如前述具體態樣中任一者之方法,其中該壓力容器包含鋼、複合材料、聚合物材料、或包含至少一種前述物之組合。 The method of any one of the preceding aspects, wherein the pressure vessel comprises steel, a composite material, a polymeric material, or a combination comprising at least one of the foregoing.

具體態樣11:一種沖洗反應器之方法,其包含:將沖洗流體流導入壓力容器,其中該壓力容器包含蒸氣注入閥和蒸氣釋放閥;當該壓力容器中的壓力達到最小值時,將第一蒸氣流通過該蒸氣注入閥並進入到該壓力容器中;當該壓力容器中的壓力達到最大值時,將第二蒸氣流通過該蒸氣釋放閥並離開該壓力容器,其中該最小值和該最大值是不同的;自該壓力容器抽出一部分該沖洗流體流;及將該部分沖洗流體流通過反應器以沖洗該反應器。 A specific aspect 11 is a method of rinsing a reactor, comprising: introducing a flow of a flushing fluid into a pressure vessel, wherein the pressure vessel comprises a vapor injection valve and a vapor release valve; when the pressure in the pressure vessel reaches a minimum value, a vapor stream passing through the vapor injection valve and into the pressure vessel; when the pressure in the pressure vessel reaches a maximum, passing a second vapor stream through the vapor release valve and exiting the pressure vessel, wherein the minimum value and the The maximum value is different; a portion of the flushing fluid stream is withdrawn from the pressure vessel; and the portion of the flushing fluid stream is passed through the reactor to flush the reactor.

具體態樣12:如具體態樣11之方法,其中該抽出的部分沖洗流體在通過該反應器前係藉由流量控制器監測。 Aspect 12: The method of Embodiment 11, wherein the extracted portion of the flushing fluid is monitored by a flow controller prior to passing through the reactor.

具體態樣13:如具體態樣11或具體態樣12之方法,其中沖洗該反應器為閉環系統。 Specific Aspect 13: The method of Concrete Aspect 11 or Aspect 12, wherein the reactor is flushed as a closed loop system.

具體態樣14:如具體態樣11-13中任一者之方法,其中該沖洗流體流包含芳族溶劑、沸點低於或等於300℃之有機液體、或包含至少一種前述物之組合,較佳者為其中該沖洗流體包含甲苯。 The method of any one of the aspects 11-13, wherein the rinsing fluid stream comprises an aromatic solvent, an organic liquid having a boiling point lower than or equal to 300 ° C, or a combination comprising at least one of the foregoing Preferably, the rinse fluid comprises toluene.

具體態樣15:如具體態樣11-14中任一者之方法,其中該第一蒸氣流包含惰性氣體,較佳者為其中該第一蒸氣流包含氮氣、甲烷氣、乙烷氣、或包含至少一種前述物之組合。 The method of any one of aspects 11-14, wherein the first vapor stream comprises an inert gas, preferably wherein the first vapor stream comprises nitrogen, methane, ethane, or A combination comprising at least one of the foregoing.

具體態樣16:如具體態樣11-15中任一者之方法,其中該壓力容器中的溫度為80℃至250℃。 The method of any one of the aspects 11-15, wherein the temperature in the pressure vessel is from 80 ° C to 250 ° C.

具體態樣17:如具體態樣11-16中任一者之方法,其中該壓力容器中的壓力的最小值為10千帕至500千帕。 The method of any one of the aspects 11-16, wherein the pressure in the pressure vessel has a minimum value of 10 kPa to 500 kPa.

具體態樣18:如具體態樣11-17中任一者之方法,其中該壓力容器中的壓力的最大值為50千帕至1000千帕。 The method of any one of the aspects 11-17, wherein the pressure in the pressure vessel has a maximum value of 50 kPa to 1000 kPa.

具體態樣19:如具體態樣11-18中任一者之方法,其中該壓力容器中的壓力的最小值與該壓力容器中的壓力的最大值相差大於或等於10千帕。 The method of any one of aspects 11-18, wherein the minimum value of the pressure in the pressure vessel differs from the maximum value of the pressure in the pressure vessel by greater than or equal to 10 kPa.

具體態樣20:如具體態樣11-19中任一者之方法,其中該沖洗流體流係藉由泵推進,其中該泵獨立於該壓力容器中的壓力操作。 The method of any one of aspects 11-19, wherein the flushing fluid flow is advanced by a pump, wherein the pump operates independently of the pressure in the pressure vessel.

具體態樣21:如具體態樣11-20中任一者之方法,其中,與用不同方法沖洗的反應器相比,每個月甲苯 的損失量被減少大於或等於45%。 The method of any one of clauses 11 to 20, wherein the toluene per month is compared to a reactor rinsed by a different method. The amount of loss is reduced by greater than or equal to 45%.

具體態樣22:如具體態樣11-21中任一者之方法,其中,與用不同方法沖洗的反應器相比,該反應器所消耗的氮量被減少大於或等於90%。 The method of any one of aspects 11-21, wherein the amount of nitrogen consumed by the reactor is reduced by greater than or equal to 90% compared to a reactor flushed by a different method.

具體態樣23:一種控制壓力容器中的壓力之系統,其包含:包含蒸氣注入閥和蒸氣釋放閥之壓力容器,其中該壓力容器係經配置成:接受導入到該壓力容器中的沖洗流體流;當該壓力容器中的壓力達到最小值時,將第一蒸氣流通過該蒸氣注入閥並進入到該壓力容器中;及當該壓力容器中的壓力達到最大值時,將第二蒸氣流通過該蒸氣釋放閥並離開該壓力容器,其中該最小值和該最大值是不同的。 Concrete aspect 23: A system for controlling pressure in a pressure vessel, comprising: a pressure vessel comprising a vapor injection valve and a vapor release valve, wherein the pressure vessel is configured to receive a flow of irrigation fluid introduced into the pressure vessel When the pressure in the pressure vessel reaches a minimum, the first vapor stream is passed through the vapor injection valve and into the pressure vessel; and when the pressure in the pressure vessel reaches a maximum, the second vapor stream is passed The vapor releases the valve and exits the pressure vessel, wherein the minimum and the maximum are different.

一般而言,本發明可替代地包含本文中所揭露的任何適當的組件、由該等組件所組成、或基本上由該等組件所組成。本發明可另外或替代地經配製,以致沒有或實質上不含用於先前技術組成物中或是另外對達成本發明之功能及/或目的為不必要的任何組件、材料、成分、佐劑或物種。針對相同組件或性質之所有範圍的端點均包括在內且可獨立組合(例如,“小於或等於25重量%、或5重量%至20重量%”的範圍包括“5重量%至25重量%”之範圍的端點及所有中間值等等)。除了較廣範圍以外的較窄範圍或更特定群組的揭露並非放棄該較廣的範圍或較大的群組。“組合”包括摻合物、混合物、合金、反應產物等等在內。再者,本文中之術語“第一”、“第二”等等不表示任何 順序、數量、或重要性,而是用於表示一個元件有別於另一個。本文中之術語“一(a)”及“一(an)”及“該(the)”不表示數量的限制,而應被解釋為包含單數及複數二者,除非在本文中另有指示或明確與上下文相牴觸。“或”意指“及/或”。如本文所用的字尾“(s)”意欲包括其所修飾的術語之單數及複數二者,從而包括一個或多個該術語(例如,膜(s)包括一或多個膜)。貫穿本說明書提到的“一個具體態樣”、“另一具體態樣”、“具體態樣”等等,意指與該具體態樣有關所描述的特定元件(例如,特點、結構、及/或特徵)被包括在本文所描述的至少一個具體態樣中,且可存在或可不存在於其他的具體態樣中。此外,應理解的是所描述的元件可以任何合適的方式組合於各種具體態樣中。 In general, the invention may alternatively comprise, consist of, or consist essentially of any suitable components disclosed herein. The invention may additionally or alternatively be formulated so as to be free or substantially free of any components, materials, ingredients, adjuvants that are used in prior art compositions or otherwise are not necessary to achieve the function and/or purpose of the invention. Or species. All ranges of endpoints for the same component or property are included and can be independently combined (eg, "less than or equal to 25% by weight, or 5% to 20% by weight" ranges include "5 to 25% by weight" "The endpoint of the range and all intermediate values, etc.". The disclosure of a narrower range or a particular group other than a broader range is not a waiver of the broader scope or larger group. "Combination" includes blends, mixtures, alloys, reaction products, and the like. Furthermore, the terms "first", "second", etc. in this document do not mean any Order, quantity, or importance, but to indicate that one component is different from the other. The terms "a", "an", "the", "the" and "the" Or clearly contradictory to the context. “or” means “and/or”. The suffix "(s)" as used herein is intended to include both the singular and the plural of the terms which are modified to include one or more of the terms (eg, the film (s) includes one or more films). Throughout the specification, "a particular aspect", "another embodiment", "an embodiment", or the like, is meant to refer to the particular elements (such as features, structures, and / or features are included in at least one specific aspect described herein and may or may not be present in other specific aspects. In addition, it is to be understood that the described elements may be combined in various embodiments in any suitable manner.

相關於數量所使用的修飾詞“約”包括所陳述的值,並且具有上下文所指定的含義(例如,包括與特定數量之測量相關聯的誤差程度)。標記“+10%”意指所示測量值可從所陳述的值的負10%的量至正10%的量。術語“前面”、“背面”、“底部”、及/或“頂部,除非另有指明,在本文中僅係用於描述方便,而非限於任何一個位置或空間方位。“隨意的”或“隨意地”意指其後所描述的事件或情況可發生或可不發生,且該描述包括該事件發生的例子及該事件不發生的例子。除非另有定義,本文所用的技術及科學術語具有與熟習本發明所屬技術人士通常所了解的相同的意義。“組合”包括摻合物、混合物、合金、反應產物等等在內。 The modifier "about" used in relation to a quantity includes the stated value and has the meaning specified by the context (eg, including the degree of error associated with a particular quantity of measurement). The designation "+10%" means that the measured value can be from the negative 10% of the stated value to the positive 10% amount. The terms "front", "back", "bottom", and/or "top, unless otherwise indicated, are used herein for convenience of description only and are not limited to any one location or spatial orientation. "arbitrary" or " "Optionally" means that the event or circumstance described thereafter may or may not occur, and that the description includes examples of the occurrence of the event and examples in which the event does not occur. Unless otherwise defined, the technical and scientific terms used herein have The same meaning as commonly understood by one of ordinary skill in the art is recognized. "Combination" includes blends, mixtures, alloys, reaction products, and the like.

除非另有指示,各前述基團可未經取代或經取代,其前提是該取代未顯著不利地影響該化合物的合成、穩定性、或用途。如本文中所用的術語“經取代”意指在指定之原子或基團上的至少一個氫被另一個基團置換,其前提是未超過所指定之原子的正常價。當取代基為側氧基(即=O),則該原子上的二個氫被置換。取代基及/或變數之組合是可允許的,其前提是該取代未顯著不利地影響該化合物的合成或用途。可存在於“經取代”位置之例示性基團包括,但不限於:氰基;羥基;硝基;疊氮基;烷醯基(例如C2-6烷醯基,例如醯基);甲醯胺基(carboxamido);C1-6或C1-3烷基、環烷基、烯基、及炔基(其包括具有至少一個不飽和鍵聯及從2至8、或2至6個碳原子之基團);C1-6或C1-3烷氧基;C6-10芳氧基,例如苯氧基;C1-6烷硫基;C1-6或C1-3烷亞磺醯基;C1-6或C1-3烷磺醯基;胺基二(C1-6或C1-3)烷基;具有至少一個芳環之C6-12芳基(例如,苯基、聯苯基、萘基、或類似物,各環為經取代或未經取代之芳族);具有1至3個分開或稠合的環及從6至18個環碳原子之C7-19芳基烷基;或具有1至3個分開或稠合的環及從6至18個環碳原子之芳基烷氧基,以苄氧基為例示的芳基烷氧基。 Unless otherwise indicated, each of the foregoing groups may be unsubstituted or substituted, provided that the substitution does not significantly adversely affect the synthesis, stability, or use of the compound. The term "substituted" as used herein means that at least one hydrogen on a specified atom or group is replaced by another group, provided that the normal valence of the specified atom is not exceeded. When the substituent is a pendant oxy group (i.e., =0), the two hydrogens on the atom are replaced. Combinations of substituents and/or variables are permissible provided that the substitution does not significantly adversely affect the synthesis or use of the compound. Exemplary groups that may be present at the "substituted" position include, but are not limited to, cyano; hydroxy; nitro; azide; alkyl fluorenyl (eg, C2-6 alkanoyl, eg, fluorenyl); Carboxamido; C 1-6 or C 1-3 alkyl, cycloalkyl, alkenyl, and alkynyl (which includes at least one unsaturated linkage and from 2 to 8, or 2 to 6 a group of a carbon atom; C 1-6 or C 1-3 alkoxy; C 6-10 aryloxy, such as phenoxy; C 1-6 alkylthio; C 1-6 or C 1-3 Alkylenesulfonyl; C1-6 or C1-3 alkanesulfonyl; an amine di( C1-6 or C1-3 )alkyl; a C6-12 aryl having at least one aromatic ring ( For example, phenyl, biphenyl, naphthyl, or the like, each ring being a substituted or unsubstituted aromatic; having from 1 to 3 separate or fused rings and from 6 to 18 ring carbon atoms a C 7-19 arylalkyl group; or an aryl alkoxy group having 1 to 3 divided or fused rings and an arylalkoxy group having from 6 to 18 ring carbon atoms, exemplified by a benzyloxy group .

所有引述之專利、專利申請案及其他參考文獻均以引用方式全部併入本文中。然而,若在本申請案中的術語與併入之參考文獻中的術語牴觸或衝突時,則出自本申請案的術語優先於出自所併入之參考文獻的衝突之術 語。 All cited patents, patent applications, and other references are herein incorporated by reference in their entirety. However, if a term in this application conflicts or conflicts with a term in the incorporated reference, the term from the present application takes precedence over the conflict from the incorporated reference. language.

雖然已描述了特定的具體態樣,但申請人或其他熟習此項技術人士可產生目前未預見或可能未預見的替代、修飾、變形、改善、及實質等效物。因此,如所提出的及如其可修改的所附申請專利範圍旨在包含所有該等替代、修飾、變形、改善、及實質等效物。 Although specific specific aspects have been described, the applicant or other skilled artisan can produce alternatives, modifications, variations, improvements, and substantial equivalents that are presently unforeseen or may be unforeseen. Accordingly, the appended claims are intended to cover all such alternatives, modifications, modifications,

10‧‧‧壓力控制方法 10‧‧‧ Pressure control method

12‧‧‧流體沖洗流 12‧‧‧ fluid flushing flow

14‧‧‧壓力容器 14‧‧‧ Pressure vessel

16‧‧‧第一蒸氣流 16‧‧‧First vapor stream

18‧‧‧蒸氣注入閥 18‧‧‧Vapor injection valve

20‧‧‧第二蒸氣流 20‧‧‧Second vapor flow

22‧‧‧蒸氣釋放閥 22‧‧‧Vapor release valve

24‧‧‧合併線 24‧‧‧ merged line

26‧‧‧泵 26‧‧‧ pump

28‧‧‧加熱器 28‧‧‧heater

30‧‧‧流量控制器 30‧‧‧Flow controller

32‧‧‧反應器 32‧‧‧Reactor

Claims (20)

一種控制壓力容器中的壓力之方法,其包含:將沖洗流體流導入壓力容器,其中該壓力容器包含蒸氣注入閥和蒸氣釋放閥;當該壓力容器中的壓力達到最小值時,將第一蒸氣流通過該蒸氣注入閥並進入到該壓力容器中;及當該壓力容器中的壓力達到最大值時,將第二蒸氣流通過該蒸氣釋放閥並離開該壓力容器,其中該最小值和該最大值是不同的。 A method of controlling pressure in a pressure vessel, comprising: introducing a flow of a flushing fluid into a pressure vessel, wherein the pressure vessel comprises a vapor injection valve and a vapor release valve; and when the pressure in the pressure vessel reaches a minimum, the first vapor is Flowing through the vapor injection valve and into the pressure vessel; and when the pressure in the pressure vessel reaches a maximum, passing a second vapor stream through the vapor release valve and exiting the pressure vessel, wherein the minimum and maximum The values are different. 如申請專利範圍第1項之方法,其中該沖洗流體流包含芳族溶劑、沸點低於或等於300℃之有機液體、或包含至少一種前述物之組合,較佳者為其中該沖洗流體包含甲苯。 The method of claim 1, wherein the rinsing fluid stream comprises an aromatic solvent, an organic liquid having a boiling point of less than or equal to 300 ° C, or a combination comprising at least one of the foregoing, preferably wherein the rinsing fluid comprises toluene . 如申請專利範圍第1或2項之方法,其中該第一蒸氣流包含惰性氣體,較佳者為其中該第一蒸氣流包含氮氣、甲烷氣、乙烷氣、或包含至少一種前述物之組合。 The method of claim 1 or 2, wherein the first vapor stream comprises an inert gas, preferably wherein the first vapor stream comprises nitrogen, methane gas, ethane gas, or a combination comprising at least one of the foregoing. . 如申請專利範圍第1或2項之方法,其中該第二蒸氣流包含呈氣相之該沖洗流體。 The method of claim 1 or 2, wherein the second vapor stream comprises the flushing fluid in a gas phase. 如申請專利範圍第1或2項之方法,其中該壓力容器中的溫度為80℃至250℃。 The method of claim 1 or 2, wherein the temperature in the pressure vessel is from 80 ° C to 250 ° C. 如申請專利範圍第1或2項之方法,其中該壓力容器中的壓力的最小值為10千帕至500千帕,且其中該壓力容器中的壓力的最大值為50千帕至1000千帕。 The method of claim 1 or 2, wherein the pressure in the pressure vessel has a minimum value of 10 kPa to 500 kPa, and wherein the pressure in the pressure vessel has a maximum value of 50 kPa to 1000 kPa. . 如申請專利範圍第1或2項之方法,其中該壓力 容器中的壓力的最小值與該壓力容器中的壓力的最大值相差大於或等於10千帕。 Such as the method of claim 1 or 2, wherein the pressure The minimum value of the pressure in the vessel differs from the maximum value of the pressure in the pressure vessel by greater than or equal to 10 kPa. 如申請專利範圍第1或2項之方法,其中該沖洗流體流係藉由泵推進,其中該泵獨立於該壓力容器中的壓力操作。 The method of claim 1 or 2, wherein the flushing fluid flow is advanced by a pump, wherein the pump operates independently of the pressure in the pressure vessel. 如申請專利範圍第1或2項之方法,其中該壓力容器包含鋼、複合材料、聚合物材料、或包含至少一種前述物之組合。 The method of claim 1 or 2, wherein the pressure vessel comprises steel, a composite material, a polymeric material, or a combination comprising at least one of the foregoing. 一種沖洗反應器之方法,其包含:將沖洗流體流導入壓力容器,其中該壓力容器包含蒸氣注入閥和蒸氣釋放閥;當該壓力容器中的壓力達到最小值時,將第一蒸氣流通過該蒸氣注入閥並進入到該壓力容器中;當該壓力容器中的壓力達到最大值時,將第二蒸氣流通過該蒸氣釋放閥並離開該壓力容器,其中該最小值和該最大值是不同的;自該壓力容器抽出一部分該沖洗流體流;及將該部分沖洗流體流通過反應器以沖洗該反應器。 A method of rinsing a reactor, comprising: introducing a flow of a flushing fluid into a pressure vessel, wherein the pressure vessel comprises a vapor injection valve and a vapor release valve; and when the pressure in the pressure vessel reaches a minimum, passing the first vapor stream Vapor is injected into the valve and into the pressure vessel; when the pressure in the pressure vessel reaches a maximum, a second vapor stream is passed through the vapor release valve and exits the pressure vessel, wherein the minimum value and the maximum value are different Extracting a portion of the flushing fluid stream from the pressure vessel; and flowing the portion of the flushing fluid through the reactor to flush the reactor. 如申請專利範圍第10項之方法,其中該抽出的部分沖洗流體在通過該反應器前係藉由流量控制器監測。 The method of claim 10, wherein the extracted portion of the flushing fluid is monitored by a flow controller before passing through the reactor. 如申請專利範圍第10或11項之方法,其中沖洗該反應器為閉環系統。 The method of claim 10, wherein the rinsing of the reactor is a closed loop system. 如申請專利範圍第10或11項之方法,其中該沖洗流體流包含芳族溶劑、沸點低於或等於300℃之有機液 體、或包含至少一種前述物之組合,較佳者為其中該沖洗流體包含甲苯。 The method of claim 10, wherein the rinsing fluid stream comprises an aromatic solvent and an organic liquid having a boiling point lower than or equal to 300 ° C. The body, or a combination comprising at least one of the foregoing, preferably wherein the rinse fluid comprises toluene. 如申請專利範圍第10或11項之方法,其中該第一蒸氣流包含惰性氣體,較佳者為其中該第一蒸氣流包含氮氣、甲烷氣、乙烷氣、或包含至少一種前述物之組合。 The method of claim 10, wherein the first vapor stream comprises an inert gas, preferably wherein the first vapor stream comprises nitrogen, methane gas, ethane gas, or a combination comprising at least one of the foregoing. . 如申請專利範圍第10或11項之方法,其中該壓力容器中的溫度為80℃至250℃,其中該壓力容器中的壓力的最小值為10千帕至500千帕,且其中該壓力容器中的壓力的最大值為50千帕至1000千帕。 The method of claim 10, wherein the temperature in the pressure vessel is from 80 ° C to 250 ° C, wherein the pressure in the pressure vessel has a minimum value of 10 kPa to 500 kPa, and wherein the pressure vessel The maximum pressure in the range is 50 kPa to 1000 kPa. 如申請專利範圍第10或11項之方法,其中該壓力容器中的壓力的最小值與該壓力容器中的壓力的最大值相差大於或等於10千帕。 The method of claim 10, wherein the minimum value of the pressure in the pressure vessel differs from the maximum value of the pressure in the pressure vessel by greater than or equal to 10 kPa. 如申請專利範圍第10或11項之方法,其中該沖洗流體流係藉由泵推進,其中該泵獨立於該壓力容器中的壓力操作。 The method of claim 10, wherein the flushing fluid flow is advanced by a pump, wherein the pump operates independently of the pressure in the pressure vessel. 如申請專利範圍第10或11項之方法,其中,與用不同方法沖洗的反應器相比,每個月甲苯的損失量被減少大於或等於45%。 The method of claim 10 or 11, wherein the amount of toluene lost per month is reduced by greater than or equal to 45% compared to a reactor flushed by a different method. 如申請專利範圍第10或11項之方法,其中,與用不同方法沖洗的反應器相比,該反應器所消耗的氮量被減少大於或等於90%。 The method of claim 10, wherein the amount of nitrogen consumed by the reactor is reduced by greater than or equal to 90% compared to a reactor flushed by a different method. 一種控制壓力容器中的壓力之系統,其包含:壓力容器,其包含蒸氣注入閥和蒸氣釋放閥,其中該壓力容器係經配置成: 接受導入到該壓力容器中的沖洗流體流;當該壓力容器中的壓力達到最小值時,將第一蒸氣流通過該蒸氣注入閥並進入到該壓力容器中;及當該壓力容器中的壓力達到最大值時,將第二蒸氣流通過該蒸氣釋放閥並離開該壓力容器,其中該最小值和該最大值是不同的。 A system for controlling pressure in a pressure vessel, comprising: a pressure vessel comprising a vapor injection valve and a vapor release valve, wherein the pressure vessel is configured to: Receiving a flow of flushing fluid introduced into the pressure vessel; when the pressure in the pressure vessel reaches a minimum, passing a first vapor stream through the vapor injection valve and into the pressure vessel; and when the pressure in the pressure vessel When the maximum is reached, a second vapor stream is passed through the vapor release valve and exits the pressure vessel, wherein the minimum and the maximum are different.
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